Development of microwave-assisted extraction followed by headspace solid-phase microextraction and gas chromatography–mass spectrometry for quantification of camphor and borneol in Flos Chrysanthemi Indici (original) (raw)
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Jpc – Journal Of Planar Chromatography – Modern Tlc, 2015
This article describes the use of microwaveassisted extraction (MAE) as a pretreatment technique for the determination of aflatoxins B 1 , G 1 , B 2 , and G 2 in grains and grain products. The optimal operation parameters, including extraction solvent, temperature, and time, were identified to be acetonitrile as the extraction solvent at 80°C with 15 min of MAE. The extracts were cleaned up using solid-phase extraction followed by derivatization with trifluoroacetic acid and were determined by liquid chromatography-fluorescence detection. A Sep-Pak cartridge was chosen over Oasis HLB and Bond Elut cartridges. By the use of aflatoxin M 1 as an internal standard, relative recoveries of the aflatoxins ranged from 90.7 to 105.7 % for corn and from 88.1 to 103.4 % for wheat, with relative standard deviations between 2.5 and 8.7 %. A total of 36 samples from local markets were analyzed, and aflatoxin B 1 was found to be the predominant toxin, with concentrations ranging from 0.42 to 3.41 μg/kg.
Pharmaceutical Methods, 2011
Background: Trigonella foenum-graecum (L.) (Fabaceae, Fenugreek) is an important ingredient of Ayurvedic and other marketed herbal formulations. Fenugreek seeds are employed in many traditional systems as an antibacterial and antidiabetic agent, gastric stimulant and galactogogue. Trigonelline, a major phytoconstituent found in fenugreek seeds, shows estrogenic, anti-diabetic and anti-invasive activity. Therefore, it is a suitable bioactive marker to establish the quality of crude drug and its formulations. Objective: To develop an efficient and effective RP-HPLC method for estimation of trigonelline from Trigonella foenum-graecum seeds and its marketed herbal formulations. Materials and Methods: Separation and detection of trigonelline was carried out on a Cosmosil CN-MS column eluted with methanol:distilled water [95:5, v/v; pH 3.5 using hydrochloric acid]. Detection was carried out at 267 nm using a Photo Diode Array detector. Fenugreek seeds and two marketed herbal formulations were subjected for HPLC analysis of Trigonelline. Results: The RP-HPLC method was validated as per ICH guidelines and the content of trigonelline in marketed polyherbal formulations such as Dibet powder and Amyron syrup was determined. The LOD and LOQ were found to be 5.00 ng/mL and 50.00 ng/mL, respectively. Detector response was linear from 100.00 to 8000.00 ng/ mL. The method was found to be simple, sensitive, accurate, reproducible and rugged. Conclusion: This work can be recommended for quality assurance and marker-based standardization of formulations containing fenugreek seeds.
Acta Chromatographica, 2012
A new, simple and reproducible HPTLC-densitometric method has been established and validated for estimation of trigonelline in leaves of Abrus precatorius L. and its herbal formulation Chatak ® using ICH guidelines. Accelerated solvent extraction (ASE) as an alternative to convention techniques was also explored for the rapid extraction. The methanol extracts of leaves, its formulation, and standard solution of trigonelline were applied on silica gel F 254 HPTLC plates and developed in twin chamber using mobile phase toluene-ethyl acetate-formic acid-methanol (2:3:1.8:3.8, v/v/v/v). The plates were scanned at 268 nm (λ max of trigonelline) using Camag TLC scanner 3 with CATS 4 software. A linear relationship was obtained between response (peak area) and amount of trigonelline in the range 40-200 ng spot −1 ; the correlation coefficient was 0.9957. ASE method has higher extraction efficiency in less time as compared to Soxhlet extraction. The HPTLC-densitometric method showed good linearity, recovery and high precision of compound. It is useful to analyze trigonelline in A. precatorius leaves and routine quality control of its marketed formulation.
Acta Chromatographica, 2012
A new, simple, and reproducible HPTLC-densitometric method has been established and validated for estimation of trigonelline in the leaves of Abrus precatorius L. and its herbal formulation Chatak ® using ICH guidelines. Accelerated solvent extraction (ASE) as an alternative to conventional techniques was also explored for rapid extraction. The methanol extracts of leaves, its formulation, and standard solution of trigonelline were applied on silica gel F 254 HPTLC plates and developed in a twin chamber using the mobile phase toluene-ethyl acetate-formic acid-methanol (2:3:1.8:3.8, v/v/v/v). The plates were scanned at 268 nm (λ max of trigonelline) using a Camag TLC scanner 3 with the CATS 4 software. A linear relationship was obtained between the response (peak area) and the amount of trigonelline in the range 40-200 ng per spot; the correlation coefficient was 0.9957. The ASE method gives higher extraction efficiency in less time compared to Soxhlet extraction. The HPTLC-densitometric method showed good linearity, recovery, and high precision. It is useful to analyze trigonelline in A. precatorius leaves and routine quality control of its marketed formulation.
Analytica Chimica Acta, 2006
Introduction -The surge of interest in naturally occurring phytochemicals with anticancer potential has led to the discovery of many molecules, one of them being thymoquinone (TQ) the bioactive constituent of the volatile oil of black seed, Nigella sativa L. (NS). Objective -The aim of the present work was to develop and validate an HPTLC method for determination of TQ in NS extracts, commercially available marketed oils, polyherbal formulations and in lipid-based oral and parenteral formulations prepared in-house. Methodology -Analysis of TQ was performed on TLC aluminium plates pre-coated with silica gel 60F-254. Linear ascending development was carried out in twin trough glass chamber, saturated with mobile phase consisting of toluene-cyclohexane (8 : 2, v/v) at ambient temperature. Camag TLC scanner III was used for the spectrodensitometric scanning and analysis in absorbance mode at 254 nm. Results -The method was found to give compact spots for TQ (Rf value of 0.28 Ϯ 0.05) and was linear over the range 100-1400 ng/spot (r 2 = 0.9921 Ϯ 0.0020). Accuracy, precision and repeatability were all within the required limits. The mean recoveries measured at three concentrations were higher than 95% with RSD Յ 3%. Conclusion -The HPTLC method developed was found to be relatively simple, rapid and accurate for the routine analysis of TQ in extracts, marketed oils, polyherbal and in-house formulations.
International Journal of Current Pharmaceutical Research
Objective: Development and validation of a simple and reliable HPLC method for determination of an alkaloid, trigonelline, in the methanolic extract of Mirabilis jalapa Linn. leaves and comparing the extraction yields of trigonelline from micro powder and ultrafine powder.Methods: The quantitation of trigonelline was carried out on a Phenomenex (Luna 5 U RP C8 (2) column, 25 cm x 4.6 mm, i.d. 5 µm), using mobile phase comprising of distilled water containing HCl (pH adjusted to 3.5) and methanol in the volume ratio of 70:30, which was delivered at the flow rate of 0.5 ml per min, at 35 °C column temperature. The detection and quantitation of trigonelline were carried out using PDA detector at the wavelength λ=264 nm.Ultra-fine powder of Mirabilis jalapa Linn. was prepared using simple stepwise powdering method. The dried leaves of Mirabilis jalapa Linn. were ground using ice jacketed domestic mixer. This powder was sieved through a BSS 85 mesh sieve and considered as a micro powder....
HPLC ANALYSIS OF TRIGONELLA FOENUM-GRAECUM SEEDS TO ASSESS PHYTOESTROGENS
Phytoestrogens are compounds synthesized in plants which mimic steroidal estrogen activity in mammals. Trigonella foenum-graecum (L.) (Fabaceae, Fenugreek) is employed in many traditional systems as an antibacterial and antidiabetic agent, gastric stimulant and galactogogue and also shows estrogenic, antidiabetic and anti-invasive activity. The present study report the separation of phytoetrogenic components of three different classes – isoflavonoids (genistein and daidzein), lignans (secoisolaricoresinol, metairesinol) and coumestrol from fenugreek seeds before and after alkaline hydrolysis. For this an HPLC system with a C-18 analytical column (100 x 4.6 mm , 5 micron) and detector of UV @ 254nm were employed. The mobile phases contained water/acetonitrile/acetic acid. The limit of detection for isoflavones is 1 µg/g, and for lignans and coumestrol 2.5 µg/g. The results pointed the presence of isoflavones (daidzein-18.2ppm, genistein-11.8ppm) and lignans (secoisolariceresinol-283.6ppm) unhydrolysed and presence of isoflavones (daidzein-100.9ppm, genistein-56.1ppm), lignans (secoisolariceresinol-1893ppm) and coumestrol (170ppm) in hydrolysed fenugreek seeds. Alkaline hydrolysis helped in better separation and quantification of phytoestrogens. High pressure liquid chromatography (HPLC) has been found to be an efficient and sensitive method for identification and quantification of different classes of phytoestrogens-isoflavonoids, lignans and coumestrol.
Iranian Journal of Pharmaceutical Research : IJPR, 2020
Mathematical algorithms offer a useful method for quantitative analysis of compounds in multi-component mixtures to overcome the overlapping problems occurred in UV spectrophotometry. The aim of this study is to develop a method for simultaneous determination of bioactive compounds in herbal dosage forms produced from fenugreek extract. A UV- spectrophotometric method based on mathematical algorithm was used to simultaneous determination of trigonelline (TRG), diosgenin (DI), and nicotinic acid (NA). The maximum absorbance (λmax) was determined to be 232.65 nm, 296.23 nm, and 262.60 nm for TRG, DI, and NA, respectively. The calibration curves showed good linearity for all analytes in the concentration range of 1–20 μg/mL (R2=0.9995, 0.9997, 0.9994 for TRG, DI and NA, respectively). The Intra- and inter-day precisions were in the range of 1.1-10.7% and 1.2-8.2%, respectively. The accuracy of the method was 96.0% for TRG, 92.9% for DI, and 104.2% for NA. The limits of detection (LOD) ...
Qualitative and Quantitative Estimation of Phytoconstituents in Trigonella Foenum Graceum
Fenugreek (Trigonella foenum-graecum) is an important spice; its dried seeds have wide application in food and beverages as a flavoring additive as well as in medicines. The objective of the present study was to evaluate the phytochemical constitution of ethanolic extract of dried plant parts (Leaf, Stem, Root and Seed) of Medicinal Herb Trigonella foenum-graecum. Qualitative and Quantitative analysis of phytochemical constituents' viz. Carbohydrate, Starch, Amino Acid, Protein, Lipid, Chlorophyll, Phenol and Alkaloid was performed by well-known test protocols available in the literature. Maximum amount of phytoconstituents was recorded in root part of plant. The results suggest that Trigonella foenum-graecum is a promising potential source of natural drug.
Phytochemical Analysis, 2007
A focused microwave-assisted extraction method was developed for the extraction of diosgenin from fenugreek (Trigonella foenum-graecum) seeds, air-dried and fresh leaves and air-dried roots. Several experimental parameters were studied, including extraction time, microwave power applied and percentage of 2-propanol in the extraction mixture as well as their interactions, in order to optimize the extraction efficiency. The two latter parameters were found to be the most important. Response surface modelling was used to predict the extraction yield of diosgenin in selected matrices. The analysis of diosgenin in crude extracts was carried out by capillary gas chromatography-mass spectrometry (GC-MS).